Potassium Carbonate → Pyridine-4-carboxaldehyde (3-Chloropropyl)imine
反応式
Cl.[Cl:2][CH2:3][CH2:4][CH2:5][NH2:6].[N:7]1[CH:12]=[CH:11][C:10]([CH:13]=O)=[CH:9][CH:8]=1.C([O-])([O-])=O.[K+].[K+]>O>[Cl:2][CH2:3][CH2:4][CH2:5][N:6]=[CH:13][C:10]1[CH:11]=[CH:12][N:7]=[CH:8][CH:9]=1参加物
5
実験手順
To 3-chloropropylamine HCl (15.1 g, 0.120 moles (hereinafter mol)) and H2O (100 mL) was added pyridine-4-carboxaldehyde (9.55 mL, 0.100 mol), then K2CO3 (8.28 g, 0.060 mol) then CH2CL2 (100 mL) and the mixture was stirred for 40 min. The phases were separated and the aq phase was extracted with additional CH2Cl2 (2×50 mL), dried (Na2SO4) and concentrated to afford 17.1 g (94%) 1H NMR (CD3Cl): d 8.69 (d, J=4.5 Hz, 2H, 8.32 (s, 1H), 8.28 (s, 1H), 7.58 (d, J=4.5 Hz, 2H), 3.71 (m, 2H), 3.63 (t, J=6 Hz, 2H), 2.24 (t, J=6 Hz, 2H). The presence of 9% of the aldehyde was evident by 1H NMR.
後処理
- customThe phases were separated
- extractionthe aq phase was extracted with additional CH2Cl2 (2×50 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customto afford 17.1 g (94%) 1H NMR (CD3Cl): d 8.69 (
出典と根拠
- ORDレコード
- ord-f5dc89926fb744dbae3dbf00f35ac64d
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06222036B1
反応ノート
読み込み中…